CN113075318A - Analysis method for chafing dish beef tallow sample in old chafing dish beef tallow production - Google Patents
Analysis method for chafing dish beef tallow sample in old chafing dish beef tallow production Download PDFInfo
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- CN113075318A CN113075318A CN202110318479.3A CN202110318479A CN113075318A CN 113075318 A CN113075318 A CN 113075318A CN 202110318479 A CN202110318479 A CN 202110318479A CN 113075318 A CN113075318 A CN 113075318A
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- 235000015278 beef Nutrition 0.000 title claims abstract description 56
- 239000003760 tallow Substances 0.000 title claims abstract description 56
- 238000004458 analytical method Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000000796 flavoring agent Substances 0.000 claims abstract description 17
- 235000019634 flavors Nutrition 0.000 claims abstract description 16
- 238000002470 solid-phase micro-extraction Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 7
- 238000010812 external standard method Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 8
- 230000005526 G1 to G0 transition Effects 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract 1
- 235000013409 condiments Nutrition 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 235000014121 butter Nutrition 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000019590 thick flavour Nutrition 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for analyzing a hot pot beef tallow sample in the production of old hot pot beef tallow, which comprises the following steps: performing odor analysis on a chafing dish beef tallow sample, extracting odor components by adopting a solid phase microextraction method and a solvent-assisted flavor evaporation method during the odor analysis, performing the odor analysis after the odor extraction, preparing 4 samples during the odor analysis of the chafing dish beef tallow sample, detecting the volatile compounds in 47 by the method in the step one, smelling by an smelling instrument, determining the odor characteristics and the smell intensity of each chromatographic peak, and measuring and quantifying the beef tallow odor components by adopting an external standard method. The method adopts a solid phase microextraction method and a solvent-assisted flavor evaporation method to extract the odor components, then carries out water bath, inserts the adsorption needle of the odor components into the injection port of GC-MS, desorbs for 5min at 250 ℃, and repeatedly detects each sample for three times, thereby being more scientific and accurate in analysis.
Description
Technical Field
The invention relates to the field of foods, in particular to a method for analyzing a hot pot beef tallow sample in the production of old hot pot beef tallow.
Background
Beef tallow is one of the most important raw materials in the hotpot condiment, the flavor of the beef tallow directly determines the flavor of the hotpot condiment, and a novel beef tallow product is produced at the beginning for frying the old hotpot condiment with a thick flavor.
Disclosure of Invention
The invention aims to provide a method for analyzing a hot pot beef tallow sample in the production of old hot pot beef tallow, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for analyzing a chafing dish beef tallow sample in the production of old chafing dish beef tallow comprises the following steps:
the method comprises the following steps: performing odor analysis on the chafing dish beef tallow sample, wherein during the odor analysis, a solid phase microextraction method and a solvent-assisted flavor evaporation method are adopted to extract odor components, and after the odor is extracted, the odor is analyzed;
step two: when the odor of the chafing dish beef tallow sample is analyzed, 4 samples are prepared, then volatile compounds in 47 are detected in total by the method in the step one, then the odor is detected by an odor detector, and the odor characteristics and the odor intensity of each chromatographic peak are measured;
step three: and measuring and quantifying the beef tallow aroma components by adopting an external standard method.
Preferably, the solvent-assisted flavor evaporation method comprises distilling under low temperature and high vacuum, and collecting distillate with cold hydrazine.
Preferably, the solid phase microextraction method is used for enriching volatile compounds by utilizing a polymer stationary phase adsorption coating with different properties coated on the surface.
Preferably, when the old chafing dish beef tallow is sampled, 7.5g of samples are respectively taken and placed in a centrifuge tube and a water bath at 60 ℃.
Preferably, when analyzing the odor, 6.0g of the old chafing dish beef tallow sample is accurately weighed in a headspace bottle by an electronic balance, and 1 is added into the bottle
The concentration of L is 1.013
Taking g/L2, 4, 5-trimethyl thiazole as an internal standard, covering a bottle cap tightly, placing the bottle cap in a water bath kettle at 60 ℃ for balancing for 30min, inserting a solid phase micro-extraction device for adsorbing at 60 ℃ for 30min, then inserting an adsorption needle adsorbing aroma components into a sample inlet of GC-MS, desorbing at 250 ℃ for 5min, and detecting each sample for three times.
Preferably, the gas chromatograph condition parameters are: setting the initial temperature to 40 ℃, keeping the temperature constant for 3min, and then heating up according to the following modes: firstly heating to 142 ℃ at the speed of 3.5 ℃/min, secondly heating to 150 ℃ at the speed of 2 ℃/min, then heating to 177 ℃ at the speed of 35 ℃/min, then heating to 200 ℃ at the speed of 6 ℃/min, finally heating to 230 ℃ at the speed of 10 ℃/min, keeping the temperature constant for 3min, using high-purity nitrogen as carrier gas, using the speed of 1.2mL/min as the constant flow rate of the carrier gas, setting the temperature of a sample inlet to be 250 ℃ and setting the state to be in a non-shunting state.
Preferably, mass spectrometry parameter conditions: the electron bombards the ion source, the electron energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is set to 150 ℃, the transmission line temperature is 28 ℃, the mass scanning range m/z is set to 40-250, and the solvent delay is 4 min.
Preferably, the aroma compound is flavored in four categories according to the analysis result.
The invention has the technical effects and advantages that: the solid-phase microextraction method and the solvent-assisted flavor evaporation method are adopted to extract the odor components, then water bath is carried out, so that the odor can be better extracted, the adsorption needle for the aroma components is inserted into the injection port of the GC-MS, desorption is carried out for 5min at 250 ℃, each sample is repeatedly detected for three times, the analysis is more scientific and accurate, and better sample analysis is facilitated.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the invention provides a method for analyzing a hot pot beef tallow sample in the production of old hot pot beef tallow, which comprises the following steps:
the method comprises the following steps:
the method comprises the following steps: performing odor analysis on the chafing dish beef tallow sample, wherein during the odor analysis, a solid phase microextraction method and a solvent-assisted flavor evaporation method are adopted to extract odor components, and after the odor is extracted, the odor is analyzed;
step two: when the odor of the chafing dish beef tallow sample is analyzed, 4 samples are prepared, then volatile compounds in 47 are detected in total by the method in the step one, then the odor is detected by an odor detector, and the odor characteristics and the odor intensity of each chromatographic peak are measured;
step three: and measuring and quantifying the beef tallow aroma components by adopting an external standard method.
The solvent-assisted flavor evaporation method comprises distilling at low temperature under high vacuum, and collecting distillate with cold hydrazine.
The solid phase microextraction method is characterized in that volatile compounds are enriched by utilizing a polymer stationary phase adsorption coating with different properties coated on the surface, and when the old chafing dish butter is sampled, 7.5g of samples are respectively placed in a centrifuge tube and placed in a water bath at 60 ℃.
When the odor is analyzed, 6.0g of the beef tallow sample of the old chafing dish is accurately weighed in a headspace bottle by an electronic balance, and 1 is added into the bottle
The concentration of L is 1.013
g/L2, 4, 5-trimethyl thiazole is taken as an internal standard, and the internal standard is placed after a bottle cap is tightly coveredBalancing in a water bath kettle at 60 ℃ for 30min, inserting a solid phase micro-extraction device to adsorb at 60 ℃ for 30min, then inserting an adsorption needle adsorbing aroma components into a sample inlet of a GC-MS, desorbing at 250 ℃ for 5min, and repeating the detection of each sample for three times, wherein the gas chromatograph conditions are as follows: setting the initial temperature to 40 ℃, keeping the temperature constant for 3min, and then heating up according to the following modes: firstly heating to 142 ℃ at the speed of 3.5 ℃/min, secondly heating to 150 ℃ at the speed of 2 ℃/min, then heating to 177 ℃ at the speed of 35 ℃/min, then heating to 200 ℃ at the speed of 6 ℃/min, finally heating to 230 ℃ at the speed of 10 ℃/min, keeping the temperature constant for 3min, using high-purity nitrogen as a carrier gas, using the speed of 1.2mL/min as the constant flow rate of the carrier gas, setting the temperature of a sample inlet to be 250 ℃ and setting the state as no-flow-splitting state: mass spectrum parameter conditions: bombarding an ion source by electrons, wherein the electron energy is 70eV, the temperature of the ion source is 230 ℃, the temperature of a quadrupole rod is set to be 150 ℃, the temperature of a transmission line is 28 ℃, the mass scanning range m/z is set to be 250, the solvent delay is 4min, and according to the analysis result, the flavors of the aroma compounds are classified into four types.
Example two:
the invention provides a method for analyzing a hot pot beef tallow sample in the production of old hot pot beef tallow, which comprises the following steps:
the method comprises the following steps:
the method comprises the following steps: performing odor analysis on the chafing dish beef tallow sample, wherein during the odor analysis, a solid phase microextraction method and a solvent-assisted flavor evaporation method are adopted to extract odor components, and after the odor is extracted, the odor is analyzed;
step two: when the odor of the chafing dish beef tallow sample is analyzed, 4 samples are prepared, then volatile compounds in 47 are detected in total by the method in the step one, then the odor is detected by an odor detector, and the odor characteristics and the odor intensity of each chromatographic peak are measured;
step three: and measuring and quantifying the beef tallow aroma components by adopting an external standard method.
The solvent-assisted flavor evaporation method comprises distilling at low temperature under high vacuum, and collecting distillate with cold hydrazine.
The solid phase microextraction method is characterized in that volatile compounds are enriched by utilizing a polymer stationary phase adsorption coating with different properties coated on the surface, and when the old chafing dish butter is sampled, 7.5g of samples are respectively placed in a centrifuge tube and placed in a water bath at 60 ℃.
When the odor is analyzed, 6.0g of the beef tallow sample of the old chafing dish is accurately weighed in a headspace bottle by an electronic balance, and 1 is added into the bottle
The concentration of L is 1.013
Taking g/L2, 4, 5-trimethyl thiazole as an internal standard, covering a bottle cap, placing the bottle cap in a water bath kettle at 60 ℃ for balancing for 30min, inserting a solid phase micro-extraction device for adsorbing at 60 ℃ for 30min, then inserting an adsorption needle adsorbing aroma components into a sample inlet of GC-MS, desorbing at 250 ℃ for 5min, and detecting each sample for three times, wherein the gas chromatograph conditions are as follows: setting the initial temperature to 40 ℃, keeping the temperature constant for 3min, and then heating up according to the following modes: firstly heating to 142 ℃ at the speed of 3.5 ℃/min, secondly heating to 150 ℃ at the speed of 2 ℃/min, then heating to 177 ℃ at the speed of 35 ℃/min, then heating to 200 ℃ at the speed of 6 ℃/min, finally heating to 230 ℃ at the speed of 10 ℃/min, keeping the temperature constant for 3min, using high-purity nitrogen as a carrier gas, using the speed of 1.2mL/min as the constant flow rate of the carrier gas, setting the temperature of a sample inlet to be 250 ℃ and setting the state as no-flow-splitting state: mass spectrum parameter conditions: bombarding an ion source by electrons, wherein the electron energy is 70eV, the temperature of the ion source is 230 ℃, the temperature of a quadrupole rod is set to be 150 ℃, the temperature of a transmission line is 28 ℃, the mass scanning range m/z is set to be 250, the solvent delay is 4min, and according to the analysis result, the flavors of the aroma compounds are classified into four types.
The solid-phase microextraction method and the solvent-assisted flavor evaporation method are adopted to extract the odor components, then water bath is carried out, so that the odor can be better extracted, the adsorption needle for the aroma components is inserted into the injection port of the GC-MS, desorption is carried out for 5min at 250 ℃, each sample is repeatedly detected for three times, the analysis is more scientific and accurate, and better sample analysis is facilitated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (8)
1. A method for analyzing a chafing dish beef tallow sample in the production of old chafing dish beef tallow is characterized by comprising the following steps:
the method comprises the following steps: performing odor analysis on the chafing dish beef tallow sample, wherein during the odor analysis, a solid phase microextraction method and a solvent-assisted flavor evaporation method are adopted to extract odor components, and after the odor is extracted, the odor is analyzed;
step two: when the odor of the chafing dish beef tallow sample is analyzed, 4 samples are prepared, then volatile compounds in 47 are detected in total by the method in the step one, then the odor is detected by an odor detector, and the odor characteristics and the odor intensity of each chromatographic peak are measured;
step three: and measuring and quantifying the beef tallow aroma components by adopting an external standard method.
2. The method for analyzing the chafing dish beef tallow sample in the production of the old chafing dish beef tallow according to claim 1, characterized in that: the solvent-assisted flavor evaporation method comprises distilling at low temperature under high vacuum, and collecting distillate with cold hydrazine.
3. The method for analyzing the chafing dish beef tallow sample in the production of the old chafing dish beef tallow according to claim 1, characterized in that: the solid phase microextraction method utilizes a high molecular stationary phase adsorption coating with different properties coated on the surface to enrich volatile compounds.
4. The method for analyzing the chafing dish beef tallow sample in the production of the old chafing dish beef tallow according to claim 1, characterized in that: when the old chafing dish beef tallow is sampled, 7.5g of samples are respectively placed in a centrifuge tube and placed in a water bath at 60 ℃.
5. The method for analyzing the chafing dish beef tallow sample in the production of the old chafing dish beef tallow according to claim 1, characterized in that: when the odor is analyzed, 6.0g of the beef tallow sample of the old chafing dish is accurately weighed in a headspace bottle by an electronic balance, and 1 is added into the bottle
The concentration of L is 1.013
Taking g/L2, 4, 5-trimethyl thiazole as an internal standard, covering a bottle cap tightly, placing the bottle cap in a water bath kettle at 60 ℃ for balancing for 30min, inserting a solid phase micro-extraction device for adsorbing at 60 ℃ for 30min, then inserting an adsorption needle adsorbing aroma components into a sample inlet of GC-MS, desorbing at 250 ℃ for 5min, and detecting each sample for three times.
6. The method for analyzing the chafing dish beef tallow sample in the production of the old chafing dish beef tallow according to claim 1, characterized in that: gas chromatograph condition parameters: setting the initial temperature to 40 ℃, keeping the temperature constant for 3min, and then heating up according to the following modes: firstly heating to 142 ℃ at the speed of 3.5 ℃/min, secondly heating to 150 ℃ at the speed of 2 ℃/min, then heating to 177 ℃ at the speed of 35 ℃/min, then heating to 200 ℃ at the speed of 6 ℃/min, finally heating to 230 ℃ at the speed of 10 ℃/min, keeping the temperature constant for 3min, using high-purity nitrogen as carrier gas, using the speed of 1.2mL/min as the constant flow rate of the carrier gas, setting the temperature of a sample inlet to be 250 ℃ and setting the state to be in a non-shunting state.
7. The method for analyzing the chafing dish beef tallow sample in the production of the old chafing dish beef tallow according to claim 1, characterized in that: mass spectrum parameter conditions: the electron bombards the ion source, the electron energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is set to 150 ℃, the transmission line temperature is 28 ℃, the mass scanning range m/z is set to 40-250, and the solvent delay is 4 min.
8. The method for analyzing the chafing dish beef tallow sample in the production of the old chafing dish beef tallow according to claim 1, characterized in that: according to the analysis results, the aroma compounds are flavored in four types.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114460182A (en) * | 2021-10-19 | 2022-05-10 | 广汉市迈德乐食品有限公司 | Qualitative and quantitative analysis method for key aroma compounds of enzymatic hydrolysis beef tallow |
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| CN110596255A (en) * | 2019-04-03 | 2019-12-20 | 北京工商大学 | Method for detecting volatile components of tomatoes and products thereof |
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2021
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| JP2014002082A (en) * | 2012-06-20 | 2014-01-09 | Chikuno Shokuhin Kogyo Kk | Quantitative method of volatile organic compound |
| CN110596255A (en) * | 2019-04-03 | 2019-12-20 | 北京工商大学 | Method for detecting volatile components of tomatoes and products thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114460182A (en) * | 2021-10-19 | 2022-05-10 | 广汉市迈德乐食品有限公司 | Qualitative and quantitative analysis method for key aroma compounds of enzymatic hydrolysis beef tallow |
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Application publication date: 20210706 |